CN108946808A - A kind of full-inorganic caesium-bismuth/antimony halide perovskite is nanocrystalline and preparation method thereof - Google Patents

A kind of full-inorganic caesium-bismuth/antimony halide perovskite is nanocrystalline and preparation method thereof Download PDF

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CN108946808A
CN108946808A CN201810659534.3A CN201810659534A CN108946808A CN 108946808 A CN108946808 A CN 108946808A CN 201810659534 A CN201810659534 A CN 201810659534A CN 108946808 A CN108946808 A CN 108946808A
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nanocrystalline
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crystal material
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CN108946808B (en
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匡代彬
王旭东
李文倩
谢瑶
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Sun Yat Sen University
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G29/00Compounds of bismuth
    • C01G29/006Compounds containing, besides bismuth, two or more other elements, with the exception of oxygen or hydrogen
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G30/00Compounds of antimony
    • C01G30/002Compounds containing, besides antimony, two or more other elements, with the exception of oxygen or hydrogen
    • C01G30/003Compounds containing, besides antimony, two or more other elements, with the exception of oxygen or hydrogen containing halogen
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/30Three-dimensional structures
    • C01P2002/34Three-dimensional structures perovskite-type (ABO3)
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    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2002/60Compounds characterised by their crystallite size
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/61Micrometer sized, i.e. from 1-100 micrometer

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Abstract

The present invention provides that a kind of full-inorganic caesium-bismuth/antimony halide perovskite is nanocrystalline and preparation method thereof, which first uses wet process or solid-phase synthesis that Cs is prepared3M2X9Micro crystal material, then by Cs3M2X9Micro crystal material carries out ultrasonic removing, obtains Cs after last centrifugal purification3M2X9It is nanocrystalline.By the optimization to material component and preparation process, nanocrystalline size can be adjustable within the scope of 2-100nm.This method is easy to operate quickly, favorable reproducibility.The Cs prepared using this method3M2X9Nanocrystalline narrow size distribution, stability are high, can be used for making photoelectric device, are applied to the fields such as solar cell, photodetector, photocatalysis and photoelectrocatalysis.

Description

A kind of full-inorganic caesium-bismuth/antimony halide perovskite is nanocrystalline and preparation method thereof
Technical field
The invention belongs to novel inorganic field of nano material preparation, and in particular to a kind of full-inorganic Cs3M2X9Perovskite nanometer Crystalline substance and preparation method thereof.
Background technique
Based on APbX3(A:Cs, CH3NH3(MA);X:Cl, Br, I) lead-based perovskite it is nanocrystalline have it is biggish absorb cut The advantages that face, high fluorescence quantum efficiency and tunable luminous within the scope of entire ultraviolet/visible light, in recent years by Very extensive concern.However, this perovskite is nanocrystalline containing toxic element lead, this perovskite nanometer is significantly limited Brilliant development, in addition to this, the nanocrystalline stability of this perovskite is also relatively poor.Therefore, synthesis is less toxic, high stability Nanocrystalline become of perovskite works as previous big research hotspot.Bismuth or antimony based perovskite body phase material have been reported in recent years, due to They have toxicity more lower than lead-based perovskite and higher stability, therefore by certain attention.But it is directed to bismuth or antimony The nanocrystalline research of based perovskite is then relatively fewer.The nanocrystalline method of this perovskite-like is synthesized at present is concentrated mainly on solvent resistant Method, hot injection method, operation is relatively complicated, and reaction condition is more harsh, and reproducibility is relatively poor.
Summary of the invention
Based on this, the present invention provides a kind of full-inorganic caesium-bismuth/nanocrystalline preparation method of antimony halide perovskite, the party Method is easy to operate quickly, favorable reproducibility.
Full-inorganic caesium-bismuth/nanocrystalline preparation method of antimony halide perovskite of the present invention the following steps are included:
S1: preparation Cs3M2X9Micro crystal material
Cs is prepared using wet process or solid-phase synthesis3M2X9Micro crystal material.
S2: preparation Cs3M2X9It is nanocrystalline
By Cs3M2X9Micro crystal material is distributed in organic solvent, ultrasonic removing is then carried out, most afterwards through centrifugal purification upper Cs is obtained in clear liquid3M2X9It is nanocrystalline.
Wherein, M is trivalent metal, one of X Cl, Br, I or a variety of mixing.
Compared with the existing technology, preparation method of the invention is by Cs3M2X9Micro crystal material carries out ultrasonic removing, can synthesize Out narrow size distribution, defect concentration it is low, without the high Cs of toxicity Pb element, stability3M2X9Full-inorganic perovskite is nanocrystalline, and It is easy to operate quick, favorable reproducibility.
Further, the M is one or both of Bi, Sb mixing.
Further, wet process described in step S1 is to aoxidize the halide metal salt containing M element, carbonate or metal Object is dissolved separately in solvent with containing caesium raw material, obtains two kinds of precursor solutions;Both precursor solutions are quickly mixed, are stirred It is largely precipitated after mixing, Cs will be obtained after precipitating drying3M2X9Micro crystal material.
Further, the solvent in the Moist chemical synthesis is ethyl alcohol, methanol, DMF, DMSO, acetonitrile, water, halogen acids equal solvent One or more of mixing.
Further, solid-phase synthesis described in step S1 be will the halide metal salt containing M element and CsX normal-temperature solid-phase Stirring is sintered to obtain Cs in 800 DEG C of following temperature3M2X9Micro crystal material.
Further, dispersing agent can be added in organic solvent described in step S2.
Further, the organic solvent is halogenated alkane, alkane, aromatic hydrocarbon, alcohols, lipid, aldehydes, one in organic acid Kind or several mixing.Such organic solvent can disperse Cs well3M2X9Micro crystal material, while will not be with Cs3M2X9Crystallite material Material reacts, changes its structure.
Further, the dispersing agent is the mixing of one or more of oleic acid, propionic acid equal solvent.It can be subtracted using dispersing agent Few nanocrystalline reunion, improves dispersion performance.
The Cs being prepared according to the above method3M2X9It is nanocrystalline to can be used for making photoelectric device, be applied to solar cell, The fields such as photodetector, photocatalysis and photoelectrocatalysis.
Detailed description of the invention
Fig. 1 is Cs3Bi2Cl9The XRD diagram of micro crystal material;
Fig. 2 is Cs3Bi2Cl9The SEM of micro crystal material schemes;
Fig. 3 is Cs3Bi2Cl9Nanocrystalline TEM figure;
Fig. 4 is Cs3Bi2Br9The XRD diagram of micro crystal material;
Fig. 5 is Cs3Bi2Br9The SEM of micro crystal material schemes;
Fig. 6 is Cs3Bi2Br9Nanocrystalline TEM figure;
Fig. 7 is Cs3Bi2I9The XRD diagram of micro crystal material;
Fig. 8 is Cs3Bi2I9The SEM of micro crystal material schemes;
Fig. 9 is Cs3Bi2I9Nanocrystalline TEM figure;
Figure 10 is Cs3Bi2I9Nanocrystalline XRD diagram;
Figure 11 is Cs3Sb2I9The XRD diagram of micro crystal material;
Figure 12 is Cs3Sb2I9The SEM of micro crystal material schemes;
Figure 13 is Cs3Sb2I9Nanocrystalline TEM figure.
Specific embodiment
The present invention prepares Cs using ultrasonic stripping means3M2X9It is nanocrystalline, can synthesize narrow size distribution, stability it is high, The Cs of opto-electronic device can be used to make3M2X9Full-inorganic perovskite is nanocrystalline, easy to operate quick, favorable reproducibility.Below by way of Specific embodiment simultaneously carrys out the technical solution that the present invention will be described in detail in conjunction with attached drawing.
Embodiment 1
S1-1: preparation Cs3Bi2Cl9Micro crystal material
By 3mmol CsCl, 2mmol BiCl3It is ground at normal temperature after mixing, obtains Cs3Bi2Cl9Micro crystal material.
S2-1: preparation Cs3Bi2Cl9It is nanocrystalline
Take 0.2g Cs3Bi2Cl9Micro crystal material is dispersed in 20mL chloroform, ultrasound 20 minutes (4 under 300W ultrasonic power Second ultrasound is spaced for 4 seconds).Then at 500 rpm after low-speed centrifugal, lower end precipitating is discarded.Then by supernatant 3000rpm's High speed centrifugation under revolving speed discards precipitating, Cs is obtained in supernatant3Bi2Cl9It is nanocrystalline.
Fig. 1 is please referred to, which is Cs3Bi2Cl9The XRD spectrum of micro crystal material, the Cs that the present invention prepares3Bi2Cl9's Characteristic diffraction peak and ICSD#2067Cs3Bi2Cl9Card image perfection coincide, it was demonstrated that has obtained pure Cs3Bi2Cl9.Please join simultaneously According to Fig. 2, which is Cs3Bi2Cl9The SEM of micro crystal material schemes.Fig. 2 shows, the Cs that the present invention prepares3Bi2Cl9Micro crystal material Size is mainly distributed between 2-8 μm.
Referring to figure 3., which is Cs3Bi2Cl9Nanocrystalline TEM figure.Fig. 3 shows, what the present invention prepared Cs3Bi2Cl9Nanocrystalline size is mainly distributed between 20-70nm.
Embodiment 2
S1-2: preparation Cs3Bi2Br9Micro crystal material
By 1.5mmol Cs2CO3, 2mmol BiBr3It is dissolved separately in 10mL hydrobromic acid, stirs 1 hour, make at 100 DEG C It is sufficiently dissolved, and obtains two kinds of precursor solutions.It filters, obtains a large amount of after two kinds of precursor solutions are quickly mixed under room temperature Precipitating, is dried to obtain Cs for precipitating in baking oven3Bi2Br9Micro crystal material.
S2-2: preparation Cs3Bi2Br9It is nanocrystalline
Take 0.2g Cs3Bi2Br9Micro crystal material is dispersed in 20mL chloroform, ultrasound 20 minutes (4 under 300W ultrasonic power Second ultrasound is spaced for 4 seconds).Then at 500 rpm after low-speed centrifugal, lower end precipitating is discarded, Cs is obtained in supernatant3Bi2Br9 It is nanocrystalline.
Referring to figure 4., which is Cs3Bi2Br9The XRD spectrum of micro crystal material, the Cs that the present invention prepares3Bi2Br9's Characteristic diffraction peak and ICSD#1142Cs3Bi2Br9Card image is coincide, it was demonstrated that has obtained pure Cs3Bi2Br9.Referring to figure 5, which is Cs3Bi2Br9The SEM of micro crystal material schemes.Fig. 5 shows, the Cs that the present invention prepares3Bi2Br9Micro crystal material size It is mainly distributed between 2-7 μm.
Fig. 6 is please referred to, which is Cs3Bi2Br9Nanocrystalline TEM figure.Fig. 6 shows, what the present invention prepared Cs3Bi2Br9Nanocrystalline size is mainly distributed between 2-5nm.
Embodiment 3
S1-3: preparation Cs3Bi2I9Micro crystal material
By 3mmol CsI, 2mmol BiI3It is dissolved separately in 10mL hydroiodic acid, is stirred 1 hour at 100 DEG C, fill it Divide dissolution, obtains two kinds of precursor solutions.It filters after two kinds of precursor solutions are quickly mixed under room temperature, is largely sunk It forms sediment, precipitating is dried to obtain Cs in baking oven3Bi2I9Micro crystal material.
S2-3: preparation Cs3Bi2I9It is nanocrystalline
Take 0.2g Cs3Bi2I9Micro crystal material is dispersed in 20mL chloroform, ultrasound (4 seconds 20 minutes under 300W ultrasonic power Ultrasound is spaced for 4 seconds).Then bottom precipitation is discarded after low-speed centrifugal at 500 rpm, Cs is obtained in supernatant3Bi2I9Nanometer It is brilliant.
Fig. 7 is please referred to, which is Cs3Bi2I9The XRD spectrum of micro crystal material, the Cs that the present invention prepares3Bi2I9Spy Levy diffraction maximum and PDF#23-0847Cs3Bi2I9Card image is coincide, it was demonstrated that has obtained pure Cs3Bi2I9.Referring to Fig. 8, The figure is Cs3Bi2I9The SEM of micro crystal material schemes.Fig. 8 shows, the Cs that the present invention prepares3Bi2I9Micro crystal material piece farmland is 2-5 μm, thickness is about 500nm.
Referring to Fig. 9 and Figure 10, the present invention has prepared the relatively pure Cs of structure3Bi2I9It is nanocrystalline, and its size About 13nm.
Embodiment 4
S1-4: preparation Cs3Sb2I9Micro crystal material
By 3mmol CsI, 1mmol Sb2O3It is dissolved separately in 10mL hydroiodic acid, is stirred 1 hour at 100 DEG C, fill it Divide dissolution, obtains two kinds of precursor solutions.It filters after two kinds of precursor solutions are quickly mixed under room temperature, is largely sunk It forms sediment, precipitating is dried to obtain Cs in baking oven3Sb2I9Micro crystal material.
S2-4: preparation Cs3Sb2I9It is nanocrystalline
Take 0.2g Cs3Sb2I9Micro crystal material is dispersed in 20mL chloroform, ultrasound (4 seconds 20 minutes under 300W ultrasonic power Ultrasound is spaced for 4 seconds).Then bottom precipitation is discarded after low-speed centrifugal at 500 rpm, Cs is obtained in supernatant3Sb2I9Nanometer It is brilliant.
Figure 11 is please referred to, which is Cs3Sb2I9The XRD spectrum of micro crystal material, the Cs that the present invention prepares3Sb2I9Spy Levy diffraction maximum and ICSD#300002Cs3Sb2I9Card image is coincide, it was demonstrated that has obtained pure Cs3Sb2I9.Referring to figure 12, which is Cs3Sb2I9The SEM of micro crystal material schemes.Figure 12 shows, the Cs that the present invention prepares3Sb2I9Micro crystal material piece farmland It is 1-5 μm, thickness is about 500nm.Please refer to Figure 13, Cs prepared by the present invention3Sb2I9Nanocrystalline size is 12-30nm.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention Range.

Claims (6)

1. a kind of full-inorganic caesium-bismuth/nanocrystalline preparation method of antimony halide perovskite, comprising the following steps:
S1: preparation Cs3M2X9Micro crystal material
Cs is prepared using wet process or solid-phase synthesis3M2X9Micro crystal material;
S2: preparation Cs3M2X9It is nanocrystalline
By Cs3M2X9Micro crystal material is distributed in organic solvent, ultrasonic removing is then carried out, most afterwards through centrifugal purification in supernatant In obtain Cs3M2X9It is nanocrystalline;
Wherein, M is trivalent metal, one of X Cl, Br, I or a variety of mixing.
2. preparation method according to claim 1, it is characterised in that: the M is one or both of Bi, Sb mixing.
3. preparation method according to claim 1, it is characterised in that: wet process described in step S1 is, by the halogen containing M element Compound metal salt, carbonate or metal oxide are dissolved separately in solvent with containing caesium raw material, obtain two kinds of precursor solutions;It will Both precursor solutions are largely precipitated after being sufficiently mixed, and will obtain Cs after precipitating drying3M2X9Micro crystal material.
4. preparation method according to claim 1, it is characterised in that: solid-phase synthesis described in step S1 is will be containing M member The halide metal salt and CsX normal-temperature solid-phase of element stir or are sintered to obtain Cs in 800 DEG C of following temperature3M2X9Micro crystal material.
5. preparation method according to claim 1, it is characterised in that: the organic solvent is halogenated alkane, alkane, fragrance The mixing of one or more of hydrocarbon, alcohols, lipid, aldehydes, organic acid.
6. a kind of full-inorganic caesium-bismuth/antimony halide perovskite is nanocrystalline, it is characterised in that: made by any one of claim 1 to 5 Preparation Method is prepared.
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Cited By (9)

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CN110482596A (en) * 2019-07-23 2019-11-22 中国计量大学 A kind of bismuth titanates nanometer piece preparation method of double lanthanide ion codopes
CN110937623A (en) * 2019-12-03 2020-03-31 吉林大学 Simple synthetic CsAgCl2Method for pure-phase inorganic non-lead perovskite
CN111790408A (en) * 2020-07-20 2020-10-20 山东大学 Bismuth/antimony-based perovskite, photocatalytic material, and preparation method and application thereof
CN112774719A (en) * 2021-01-22 2021-05-11 暨南大学 Novel limited-area inorganic perovskite Cs3Bi2Br9Photocatalytic film and preparation method and application thereof
CN112798545A (en) * 2019-11-13 2021-05-14 中国科学院大连化学物理研究所 Inorganic perovskite material with continuously adjustable absorption spectrum and preparation and application thereof
CN113134376A (en) * 2021-04-19 2021-07-20 铜陵博雅渡业新材料科技有限公司 Cs3Bi2Cl9(PQDs) supported nanosheet self-assembled bismuth oxycarbonate microsphere visible-light-driven photocatalyst and preparation method thereof
CN114437722A (en) * 2022-01-27 2022-05-06 江西理工大学 Rare earth-based perovskite CsTmCl3Microcrystalline material and preparation method and application thereof
CN114560500A (en) * 2022-02-18 2022-05-31 河北工业大学 Non-lead perovskite material and preparation method and application thereof
CN114590836A (en) * 2022-03-08 2022-06-07 中国科学技术大学 Lead-free halide perovskite nanocrystal, liquid-phase synthesis method thereof and application of perovskite nanocrystal in photoelectric detector

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Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110482596A (en) * 2019-07-23 2019-11-22 中国计量大学 A kind of bismuth titanates nanometer piece preparation method of double lanthanide ion codopes
CN110482596B (en) * 2019-07-23 2022-07-08 中国计量大学 Preparation method of double lanthanide ion co-doped bismuth titanate nanosheet
CN112798545B (en) * 2019-11-13 2022-03-29 中国科学院大连化学物理研究所 Inorganic perovskite material with continuously adjustable absorption spectrum and preparation and application thereof
CN112798545A (en) * 2019-11-13 2021-05-14 中国科学院大连化学物理研究所 Inorganic perovskite material with continuously adjustable absorption spectrum and preparation and application thereof
CN110937623A (en) * 2019-12-03 2020-03-31 吉林大学 Simple synthetic CsAgCl2Method for pure-phase inorganic non-lead perovskite
CN111790408A (en) * 2020-07-20 2020-10-20 山东大学 Bismuth/antimony-based perovskite, photocatalytic material, and preparation method and application thereof
CN112774719A (en) * 2021-01-22 2021-05-11 暨南大学 Novel limited-area inorganic perovskite Cs3Bi2Br9Photocatalytic film and preparation method and application thereof
CN112774719B (en) * 2021-01-22 2023-08-04 暨南大学 Limited domain inorganic perovskite Cs 3 Bi 2 Br 9 Photocatalytic film and preparation method and application thereof
CN113134376A (en) * 2021-04-19 2021-07-20 铜陵博雅渡业新材料科技有限公司 Cs3Bi2Cl9(PQDs) supported nanosheet self-assembled bismuth oxycarbonate microsphere visible-light-driven photocatalyst and preparation method thereof
CN113134376B (en) * 2021-04-19 2023-01-31 铜陵博雅渡业新材料科技有限公司 Cs 3 Bi 2 Cl 9 (PQDs) supported nanosheet self-assembled bismuthyl carbonate microsphere visible-light-driven photocatalyst and preparation method thereof
CN114437722A (en) * 2022-01-27 2022-05-06 江西理工大学 Rare earth-based perovskite CsTmCl3Microcrystalline material and preparation method and application thereof
CN114437722B (en) * 2022-01-27 2023-05-16 江西理工大学 Rare earth based perovskite CsTmCl 3 Microcrystalline material and preparation method and application thereof
CN114560500A (en) * 2022-02-18 2022-05-31 河北工业大学 Non-lead perovskite material and preparation method and application thereof
CN114560500B (en) * 2022-02-18 2024-04-09 河北工业大学 Leadless perovskite material and preparation method and application thereof
CN114590836A (en) * 2022-03-08 2022-06-07 中国科学技术大学 Lead-free halide perovskite nanocrystal, liquid-phase synthesis method thereof and application of perovskite nanocrystal in photoelectric detector

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